Validamine synthesis
- Product Name:Validamine
- CAS Number:32780-32-8
- Molecular formula:C7H15NO4
- Molecular Weight:177.2
38665-10-0
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Yield:32780-32-8 41.1 g
Reaction Conditions:
Stage #1: (+)-validoxylamine Awith N-Bromosuccinimide;water at 25; for 4 h;
Stage #2: with hydrogen;palladium in water at 50; under 37503.8 Torr; for 4 h;Temperature;Pressure;
Steps:
1.1; 1.2 Example 1:
(1) Add 100g well to a 1000mL flaskGamexylamine A,80g NBS and 500mL deionized water,The reaction was stirred at 25 °C for 4 h. After the reaction was diluted with water 10 times, the ion exchange column (D113,Hangzhou Zhengguang Resin Co., Ltd., 1500mL, NH4+ type), washed with 5000mL deionized water,Then elute with 4500mL 0.5mol/L ammonia water.Collecting the fraction of chlorenylmyrmine and argentillin,Concentrate to dryness under reduced pressure to obtain 45.2 g of sample.(2)The mixture was dissolved in 500 mL of water and placed in a 1000-mL hydrogenation reactor.At the same time, put 5g of supported Pd catalyst (Conner New Material (Hangzhou) Co., Ltd.),Hydrogen was added to a pressure of 5 MPa and reacted at 50° C. for 4 h. After the reaction is over,The solid was filtered off and diluted 10-fold with deionized water onto an ion exchange column (ibid.).Washed with 5000 mL of deionized water,Then elute with 4500mL 0.5mol/L ammonia water.Collect the part of the mixture of Jinggang amines,Concentrate under reduced pressure and vacuum dry (45°C) to obtain 41.1 g of Jinggangmycin sample.HPLC detectionThe purity is 96.4%.
References:
CN107501102,2017,A Location in patent:Paragraph 0020-0022; 0024; 0028; 0032; 0036; 0040; 0044
1316231-06-7
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32780-32-8
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151693-59-3
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32780-32-8
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